CN1990104A - Molecular sieve catalyst, preparing method and use thereof - Google Patents
Molecular sieve catalyst, preparing method and use thereof Download PDFInfo
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- CN1990104A CN1990104A CN 200510136597 CN200510136597A CN1990104A CN 1990104 A CN1990104 A CN 1990104A CN 200510136597 CN200510136597 CN 200510136597 CN 200510136597 A CN200510136597 A CN 200510136597A CN 1990104 A CN1990104 A CN 1990104A
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- molecular sieve
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Abstract
A modified molecular sieve catalysts used for olefin aromatization reaction, make up of molecular sieve and adhesive, the adhesive weight is 20 ~ 80% of the catalyst weight. The molecular sieve park in the alkaline solution that the concentration of 0.01 - 5M at room temperature to 100 Deg C for 0.1-50 hours; After washing, drying, and extrusion molding with the adhesive, via ammonia exchange, drying, roasting under 400 ~ 1000 Deg C, obtaining the goal product. Compare With ordinary untreated catalyst, the invention of the modified molecular sieve catalysts show good mixed reaction olefin aromatization Stability.
Description
Technical field
The present invention relates to a kind of modified molecular sieve catalyst.
The invention still further relates to the preparation method of above-mentioned molecular sieve catalyst.
The invention still further relates to the application of above-mentioned molecular sieve catalyst.
Background technology
Directly burn as domestic fuel at present, yet, need improve potential using value as the liquefied gas of oil product along with non-renewable petroleum-based energy is in short supply day by day from the mixed light-hydrocarbon of refinery especially liquefied gas major part.Along with the raising of environmental requirement, liquefied petroleum gas more and more comes into one's own as clean fuel for vehicle simultaneously, and directly contains a large amount of alkene in the liquefied gas from the refinery, can not be directly as vehicle fuel.Isobutene in the liquefied gas can be used as the raw material of etherificate, and 1-butylene in the liquefied gas and 2-butene content are still very high.Along with " enforcement of West-east Gas engineering will be superfluous as the domestic fuel liquefied gas.The aromatization of the alkene in the lower carbon number hydrocarbons of refinery especially liquefied gas both can solve the superfluous problem of liquefied gas, also can produce the high-octane gasoline that meets new standard and qualified motor liquified gas simultaneously.
Patent CN98116429 solid superacid as catalyst iso-butane and butene alkylated production clean gasoline.CN94120022 uses solid heteropoly acid catalyzing iso-butane alkane and butene alkylated production clean gasoline among the CN94 120018.
Patent CN87103258 is a catalyst with the ZSM-5 zeolite, and polymerization of low-carbon olefin is produced gasoline, at 980KPa, and 361 ℃ of reaction temperatures, air speed 1.80h
-1, yield of gasoline is 52.7%, Study of Gasoline method octane number is 91.9.
And, adopt light-hydrocarbon aromatized technology to produce benzene, toluene and dimethylbenzene at present mostly about the utilization of lighter hydrocarbons, by-product hydrogen simultaneously.Catalyst generally adopts the ZSM-5 sieve peg-raking catalyst of ZSM-5 or modification, and reaction temperature generally adopts pyroreaction.
Typical light-hydrocarbon aromatized technology is the CYCLAR technology of UOP and BP company, and catalyst adopts metal-modified ZSM-5, considers the easy carbon distribution of catalyst and inactivation has adopted moving bed cyclic regeneration technology.Though realized continued operation, the investment cost height, operation easier is big, is difficult to promote at home.In order to adapt to the requirement of fixed bed, improve the stability of ZSM-5 aromatisation, people improve catalyst from the following aspects.
In order to reduce the carbon distribution of catalyst, patent CN1062100A discloses a kind of aromatizing catalyst for light hydrocarbon that contains noble metal, and active component is platinum, zinc or gallium, and carrier is ZSM-5 zeolite and/or ZSM-11 and SiO
2And/or Al
2O
3Mixture on fixed bed reactors, under 500 ℃, normal pressure, under 2.0 air speeds, carries out the reaction of lighter hydrocarbons aromatization, and the one way life-span is 200 hours, and aromatics yield is 50%.
Patent CN1070847A then discloses a kind of HZSM-5 catalyst with gallium, zinc, platinum modification, this activity of such catalysts constituent content is a gallium 0.5～2.0%, zinc 0.5～2.0, platinum 0.1～0.5%, all the other are 40～100 HZSM-5 for silica alumina ratio, and the ratio of active component and bonding agent is 70: 30.The preparation method is flooded gallium at HZSM-5 earlier, and extruded moulding is being handled 3h, final impregnating zinc and platinum with 15～20% water vapour air stream down at 600～700 ℃ then.Normal pressure, fixed bed reactors, 500 ℃, air speed 0.5h
-1Carry out C down,
5～C
8Aromatisation, in 240 hours catalyst one way life-spans, aromatics yield is not less than 40wt%.
In catalyst, add noble metal, can reduce the generation of carbon distribution, but the cost of catalyst can increase greatly, and noble metal is very responsive to the sulphur in the raw material, and sulfur poisoning easily takes place.Patent CN1063121A discloses a kind of with Al and/or rare earth modified aromatized catalyst, with La (NO
3)
3Or Ce (NO
3)
2Solution direct impregnation H-ZSM-5.
Patent CN1058284C then discloses a kind of with Zn and rare earth modified H-ZSM-5 aromatizing catalyst for light hydrocarbon, and the introducing of Zn is with (Zn (NH
3)
4)
2+Complex ion solution is maceration extract, catalyst is carried out high-temperature water vapor handle, and at 520～550 ℃, weight space velocity is 0.6～1.5 hour
-1Condition under, to mixed C
4Aromatization, aromatics yield is 300～450 hours greater than 40% one way life-span.
Although very big improvement has been arranged on the above aromatization of low carbon hydrocarbon activity of such catalysts, because reaction is at high temperature carried out, inevitably produce a large amount of methane and ethane, reduced the economic benefit of aromatisation.
Summary of the invention
The object of the present invention is to provide a kind of modified molecular sieve catalyst.
Another purpose of the present invention is to provide the method for the above-mentioned catalyst of preparation.
For achieving the above object, catalyst provided by the invention is a kind of fixed bde catalyst of high stability, is made up of molecular sieve and bonding agent, and wherein the content of bonding agent accounts for 20～80wt% of catalyst weight.
Molecular sieve among the present invention can be MCM-22, ZSM-5, ZSM-11, one or more in the ZSM-22 molecular sieve.
Bonding agent among the present invention is one or more of clay, kaolin, aluminium oxide, Ludox, aluminium colloidal sol.
The method of the above-mentioned catalyst of preparation provided by the invention, its step is as follows:
It is the aqueous slkali of 0.01-5M that used molecular sieve is placed concentration, room temperature～100 ℃ following the processing 0.1-50 hour; Through washing, drying, with the bonding agent extruded moulding that accounts for gross weight 20～80%, through the ammonia exchange, drying, 400～1000 ℃ of following roastings get target product H-type molecular sieve catalyst.
Alkaline concentration among the present invention is preferably 0.05～0.3M.
Treatment temperature among the present invention is preferably 50～80 ℃.
Processing time among the present invention is preferably 2～10 hours.
Target product among the present invention carries out hydrothermal treatment consists at 400～700 ℃.
Catalyst provided by the invention can be used for the mixed olefins aromatization, and alkene in the liquefied gas or the alkene in the light petrol are converted into the high-octane gasoline with low benzene content under relatively low temperature.Compare with unmodified catalyst, the catalyst of this invention shows higher reaction stability.
The specific embodiment
Below by example in detail the present invention is described in detail.
The mixing lower carbon number hydrocarbons raw material that following example is used composed as follows: (wt%)
Propylene 0.23%, iso-butane 35.23%, 1-butylene 13.57%, anti-2-butylene 23.60%, propane 1.23%, normal butane 12.36% is along 2-butylene 13.78%.
Embodiment 1
The preparation typical catalyst:
1) Na type ZSM-5 molecular sieve (silica alumina ratio is 55) after the roasting and 30%wt SB powder are (promptly, styrene-butadiene, adopt German imported product) behind the extruded moulding, dry, roasting, carry out ammonia exchange, roasting again, obtain used H-type molecular sieve catalyst, the reactor procatalyst of packing into is ground into 20-40 purpose particle, is designated as P.
2) 5g step 1 gained catalyst is positioned in the fixed bed reactors that internal diameter is 10mm continuous-flow, the liquefied gas raw material is at 350 ℃, 5atm, 2h
-1Contact catalyst under the weight space velocity condition, reaction result such as table 1.
Prepare catalyst of the present invention:
Na type ZSM-5 molecular sieve (silica alumina ratio is 55) 20g after the roasting, place the NaOH solution of 1000ml, 0.2M, 80 ℃ are stirred after 6 hours down, cool to room temperature, then filter, wash to neutral, after the drying, with 30%wt SB powder (German import) extruded moulding, NH is carried out in dry, 800 ℃ of roastings again
+ 4Exchange, roasting obtain the used H-type catalyst of the present invention, are designated as AT.
Need to prove that the present invention prepares washing in the catalyst, drying, roasting etc. and is techniques well known, does not therefore describe in detail one by one.
Above-mentioned two kinds of catalyst are reacted reaction result such as table 1 under identical condition.
As can be seen from Table 1, compare with the catalyst P of not process modification, the initial aromatization activity of the catalyst A T after the alkali treatment does not reduce, and slightly raise on the contrary, and aromatization stability is greatly improved.In addition, this processing method has increased the mesopore and the external surface area of catalyst, and the acidity of catalyst and micropore significantly do not change.With unmodified catalyst ratio, after the reaction, the carbon deposition quantity on the modified catalyst of the present invention does not have obvious variation.
Table 1
| Reaction time (h) | Butene conversion (%) | Arene content in the liquid (wt%) | ||
| Catalyst P | Catalyst A T | Catalyst P | Catalyst A T1 | |
| 2 | 99.9 | 99.9 | 61.95 | 63.61 |
| 7 | 99.5 | 99.89 | 56.74 | 61.89 |
| 13 | 99.1 | 99.78 | 48.01 | 60.98 |
| 13 | 98.4 | 99.45 | 38.56 | 61.21 |
| 29 | 96.5 | 99.23 | 26.7 | 60.01 |
| 35 | 92.1 | 99.14 | 21.6 | 56.98 |
| 40 | 88.6 | 98.59 | 16.9 | 55.46 |
Example 2
Above catalyst P and AT pass through steam treatment respectively, and the steam treatment temperature is 530 ℃, and the processing time is 3h, and the catalyst of gained is remembered respectively and made P-530 and AT-530.Remove reaction temperature and bring up to 365 ℃, other reaction conditions are identical with example 1, reaction result such as table 2.
Table 2
| Reaction cumulative time/h | Butene conversion % | Arene content wt% in the liquid | ||
| P-530 | AT1-530 | Catalyst P | Catalyst A T1 | |
| 3 | 99.9 | 99.9 | 61.95 | 62.9 |
| 9 | 99.5 | 99.89 | 60.76 | 62.19 |
| 19 | 99.1 | 99.78 | 58.59 | 62.38 |
| 24 | 98.4 | 99.45 | 56.48 | 62.56 |
| 29 | 98.79 | 99.23 | 53.62 | 61.96 |
| 33 | 97.93 | 99.14 | 49.87 | 58.65 |
| 42 | 97.16 | 98.59 | 44.59 | 57.98 |
| 47 | 97.25 | 99.1 | 40.89 | 58.13 |
| 53 | 95.31 | 98.3 | 38.76 | 57.67 |
| 60 | 90.19 | 98.42 | 35.26 | 56.98 |
As can be seen from Table 2, catalyst P and AT are through high-temperature water heat treatment, and modified catalyst AT-530 of the present invention shows the better aromatisation stability than P-530, and the carbon deposition quantity on the catalyst is still almost equal.
Claims (10)
1, a kind of modified molecular sieve catalyst that is used for the alkene aromatization is made up of molecular sieve and bonding agent, and wherein bonding agent accounts for 20～80% of catalyst weight.
2, by the described molecular sieve catalyst of claim 1, it is characterized in that described molecular sieve is one or more in MCM-22, ZSM-5, ZSM-11, the ZSM-22 molecular sieve.
3,, it is characterized in that described bonding agent is one or more of clay, kaolin, aluminium oxide, Ludox, aluminium colloidal sol by the described molecular sieve catalyst of claim 1.
4, it is the aqueous slkali of 0.01-5M that a kind of method for preparing the described molecular sieve catalyst of claim 1, used molecular sieve place concentration, room temperature～100 ℃ following the processing 0.1-50 hour; Through washing, drying, with the bonding agent extruded moulding, through the ammonia exchange, drying, 400～1000 ℃ of following roastings get target product.
5, by the described preparation method of claim 4, it is characterized in that described aqueous slkali is NaOH, KOH or NH
3.H
2O solution, the perhaps carbonate solution of K or Na.
6, by the described preparation method of claim 4, it is characterized in that described alkaline concentration is 0.05～0.3M.
7, by the described preparation method of claim 4, it is characterized in that described treatment temperature is 50～80 ℃.
8, by the described preparation method of claim 4, it is characterized in that the described processing time is 2～10 hours.
9, by the described preparation method of claim 1, it is characterized in that described target product carries out hydrothermal treatment consists at 400～700 ℃.
10, the described molecular sieve catalyst of claim 1 is used for alkene aromatization condition and is: 250～450 ℃, and pressure 0.5～50atm, weight space velocity 0.1～10h
-1Reacting used raw material is the light petrol that is rich in the liquefied gas of alkene or is rich in alkene.
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| CN 200510136597 CN1990104A (en) | 2005-12-30 | 2005-12-30 | Molecular sieve catalyst, preparing method and use thereof |
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| CN102557071A (en) * | 2012-01-06 | 2012-07-11 | 中国石油大学(华东) | ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof |
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